Process of making cyanogen compounds.



H. FOERSTERLING & H. PHILIPP.

PROCESS OF MAKING CYANOGEN COMPOUNDS.

APPLICATION FILED JUNE 2. I910- RENEWED JUNE 21. l9l6.

1 9 1 77 Patented Feb. 6, 1917.

ED STATE PATEN QED- HANS FOERSTERLING AND. HERBERT lPI-IILIP P, OF PERTHAMBOY, NEW JERSEY,

ASSIGNORS TO THE ROESSLER Na Y.,A CORPORATION OF NEW YORK.

& HASSLACHER CHEMICAL CO., 0F NEW YORK,

PROCESS OF MAKING CYANOGEN COMPOUNDS.

emme.

Specification of Letters Patent.

Patented lFePoa 6, 1911?.

Application filed June 2, 1910, Serial No. 564,672. Renewed June 21,1916. Serial No. 105,086.

To all whom it may concern: 1

Be it known that we, HANS FOERSTERLING, a subject of the Emperor ofGermany, and HERBERT PHiLIPP, a subject of the King of Great Britain,both residing at Perth Amboy, Middlesex county, New Jersey, haveinvented certain new and useful Improvements in Processes of MakingCyanogen Compounds, of which the following 1s a specification.

This invention relates to a method of making cyanogen compounds byvaporizing a metal capable of forming cyanogen compounds and reactingthe vaporized metal with nitrogenousand carbonaceous matter.'

In United States Letters Patent No.

993,391, dated May 30, 1911, McNitt has disclosed a method for reducingmetals, based on the electrolysis of metallic compounds, the alloying ofthe separated metal with the cathode metal and the separating of thetwo-metals by passing a current of inert gas through the hot alloywhereby the more volatile metal is vaporized.

, We have found that, with a metal capable of forming cyanogen compoundsand with nitrogen as the inert gas, the passing of the volatilemetal-vapors together with the nitrogen through a furnace containingcarbon, easily forms cyanogen compounds.

in United States Patent No. 914,100, Acker has disclosed a process ofproducing cyanogen compounds by electroly'zing a molten compound of ametal, alloying the separated metal with the cathode metal, removing thealloy from the electrolytic cell and reacting on the alloyed metal withnitrogenous and carbonaceous reagents.

Our method differs from Ackers in :that we first separate the volatilemetal from the cathode metal and then bring the volatile metal incontact with nitrogenous and carbonaceous matter.

In the following we have described, in connection with the accompanyingdrawing, one way of practising our process, the features thereof beingmore particularly point ed out hereinafter in the claims.

The drawing is a diagrammatic sectional view of a form of apparatusillustrating'one way of carrying out our processand in connectiontherewith we shall describe our process as applied for instance to theproduction of an alkali cyanid such as sodium cyanid.

We electrolyze sodium chlorid in the presence of a suitable cathodemetal such as lead, in any well-known manner and obtain an alkali metalalloy, specifically sodium lead alloy, as described by McNitt in hisUnited States Patent No. 993,391 for instance. As McNitt has fullydescribed his cell in the patent referred to, We shall not describe ithere further than that the refer,-

ence numeral 1 indicates the electrolytic chamber.

2 indicates the furnace chamber.

3 indicates a transverse partition extending from side to side of thechamber 1 leaving anopening 4 at one end between the end of thepartition and the wall of chamber 1, the other end of partition 3 being.bent so as to form a seal 5 into which depends end wall 6 of chamber 1.

7 7 indicate the anodes, 8 the cathode met al, molten lead for instance,9 the electrolyte, sodium chlorid for instance, 10 a pipe for conductingan inert gas, such as nitrogen, to a point beneath the surface of thecontents of furnace chamber 2 and 11 indicates a furnace for heatingfurnace chamber 2.

lln the operationlof the cell as described the sodium is separated fromthe chlorin, which latter passes ofi' and is alloyed with the cathodemetal. llhe alloy is caused to circulate out of chamber 1 through seal 5into furnace chamber 2, as described by -McNitt, where it is maintainedat a suitable temperature and subjected to the action of the inert gaswhich passes in the usual manner,

through the same, the gas carrying the so- I diurn vapor throughconnection12 into retort 13, heated in any suitable manner not shown),the remaining portion of the modten alloy, freed from some or all of thesodium, being drawn through channel 1% and open:-

ing 4 into chamber 1 where the residual metalv again serves as thecathode and the operation repeated.

The sodium leadalloy is kept at such a temperature in chamber 2 as topermit the inert gas, specifically nitrogen, to be introduced thereinwithout reaction therewith so that the gas may carry 0d the sodium vaporas a metal per se as described. The retort 13 is kept at such "atemperature that the sodium vapors combine in the presence of nitrogenand charcoal to form sodium cyanid. v

The carbonaceous material in retort 3 rests on a grate 15 through whichthe alkali cyanid, formed as described, drips into the drum 16 of theretort and is thence permitted to flow 0% in any suitable manner, asthrough outlet 17. Fresh charcoal is added'from time to time asrequired. Very little fuel is required in practising our process asp-theformat-ion of cyanid takes place at not much above the temperature atwhich the electrolysis takes place llt is to be understood that we donot limit ourselves to the process as described. The metal from whichthe cyanid is formed may be produced without intermediate formation ofan alloy, for instance sodium, chlorid may be electrolyzed by adiaphragm process and the sodium directly vaporized with ni-= trogen;instead of blowing nitrogen into the alloy, hydrogen or other inert gasmay be used and the process may be carried out in two steps if desired.

Whermwe use the term sodium salt we intend to include as well a sodiumsalt mixture.

What we claim as our invention is:

1. The method of making cyanogen compounds consisting in vaporizing ametal, capable of forming cyanogen compounds, from an alloy containingthe same, and reacting upon the vaporized metal with nitrogenous andcarbonaceous matter. 0

2. The method of making cyanogen compounds consisting in vaporizing ametal, ca pable of forming cyanogen compounds, from an alloy containingthe same, by blowing an inert gas through the molten alloy and reactingupon the vapors with nitrogenous and carbonaceous matter. I

3 The method of making cyanogen cornpounds consisting in vaporizing ametal,capable of forming cyanogen compounds, from an alloy containingthe same, by passing a currentof nitrogen through the molten alloy andreacting upon the vapor mixturewith carbonaceous matter.

4i. The method of making cyanogen compounds consisting in electrolyzinga metallic compound containing a metal capable of forming cyanogencompounds, alloying said metal with another metal, separating the a armac;

ing the first gietal in the presence of a current of nitrogen andreacting upon the vapor mixture with carbonaceous matter.

6., The method of making sodium cyanid consisting in vaporizing thesodium from an alloy and reacting upon the sodium vapors withnitrogenous and carbonaceous matter.

7. The method of making sodium cyanid consisting in vaporizing thesodium from an alloy in the presence of a current of nitrogen andreacting upon the sodium nitrogen vapors with carbonaceous matter.

8. The method of making sodium cyanid consisting in electrolyzing asodium salt, alloying the sodium formed with another metal, separatingthe sodium from the alloy by vaporization and reacting upon the sodiumvapors with nitrogenous and carbonaceous matter.

t. The method of making sodium cyanid consisting in electrolyzing asodium salt, alloying the sodium formed with another metal, separatingthe sodium from the alloy in the presence of a current of nitrogen andreacting upon the sodium nitrogen vapors with carbonaceous matter.

10. The method of making sodium cyanid consisting in electrolyzingsodium chlorid,

alloying the sodium with a cathode metal, 7

separating the sodium from the alloy by vaporization and reacting uponthe sodium vapors with nitrogenous and carbonaceous matter.

11. The method of making sodium cyanid consisting in electrolyzingsodium chlorid, alloying the sodium with lead, separating the sodiumfrom the alloy by vaporization and reacting upon the sodium vapors withnitrogenous and carbonaceous matter.

12. The method of making sodium cyanid alloying the sodium with acathode metal,

emme separating the sodium from the alloy by current of inert gas andreacting upon the sodium with nitrogen and charcoal.

17. The method of making sodium cyanid consisting in electrolyzingsodium chlorid,

alloying the sodium with lead, separating the sodium from the alloy by acurrent of inert gas and reacting upon the sodium with nitrogen andcharcoal.

18. The method of making cyanogen compounds consisting in electrolyzinga molten compound of a metal capable of forming nitrogen compounds,alloying the separated metal with a cathode metal, removing the alloyedcathode metal and metal capable of forming a nitrogen compound andtreating the last mentioned metal to separate at least a part of thesame from the alloy as a metal per se and treating said separated metalwith nitrogenous and carbonaceous matter.

19. The method of making cyanogen com= pounds consisting inelectrolyzing a molten compound of a metal capable of forming nitrogencompounds, alloying the separated metal with a cathode metal, removingthe alloyed cathode metal and metal capable of forming nitrogencompounds, separating at least a part of the last mentioned metal as ametal per se, from the alloy, treating said separated metal withnitrogenous and carbonaceous matter and returning the residual metal tothe cathode.

20. The method of making cyanogen compounds consisting in continuouslyelectrolyzing a molten compound of a metal capable of forming nitrogencompounds, alloying the separated metal with a cathode metal, removingthe alloy, separating as a metal per se the constituent metal of saidalloy which is capable of forming nitrogen compounds, from said alloy,reacting on the so'separated metal at a higher tempera:

ture with nitrogenous and carbonaceous reagents and returning theresidual metal to the cathode.

21. The method of making cyanogen compounds consisting in continuouslyelectrolyzing a molten compound of a metal capable of forming nitrogencompounds, alloying the separated metalwith a cathode metal, removingthe alloy, separating as a metal per se the constituent metal of saidalloy which is capable of forming nitrogen compounds, from said alloyand treating said separated metal with nitrogenous and carbonaceousmatter.

22. The method of making cyanogen compounds consisting in continuouslyelectrolyzing a molten compound of a metal capable of forming nitrogencompounds, alloying the separated metal with a cathode metal, removingthe alloy, separating as a metal per 86 in the form of a vapor theconstituent metal of said alloy which is capable of forming nitrogencompounds, from said alloy and treating said separated metal in the formof a vapor with nitrogenous and carbonaceous matter.

23. The method of making cyanogen compounds consisting in continuouslyelectrolyzing a molten compound of a metal'capable of forming nitrogencompounds, alloying said metal with another metal, removing the alloy,separating as a metal per se the constituent metal of said alloy whichis capable of forming nitrogen compounds, from said alloy and treatingsaid separated metal with nitrogenous and carbonaceous matter.

24. The method of making cyanogen compounds consisting in continuouslyelectrolyzing a molten compound of a metal capable of forming nitrogencompounds, alloying said metal with another metal, removing the alloy,separating as a metal per se in the form of a vapor the constituentmetal of said alloy which is capable of forming nitrogen compounds, fromsaid alloy and treating said separated metal in the form of a vapor withnitrogenous and carbonaceous matter.

25. The method of making alkali-metal cyanogen compoundsconsisting incontinuously electrolyzing a molten compound of the alkali-metal,alloying the separated alkali-metal with a cathode metal, removing thealloy, separating as a metal per se the alkali-metal from said alloy,reacting on said separated metal with a nitrogenous and a carbonaceousreagent and returning the residual metal to the cathode.

26. The method of making cyanogen compounds consisting in electrolyzinga molten compound. of a metal capable of forming nitrogen compounds,alloying the separated metal with a cathode metal, removing the alloy,separating as a metal per se the constituent metal of said alloy whichis capable of forming nitrogen compounds, from said alloy, reacting onthe so-separated metal with nitrogenous and carbonaceous reagents andreturning the residual metal to the cathode.

27. The method of making alkali-metal cyanogen compounds consisting inelectrolyzing a molten compound of the alkali-- carbonaceous reagent andreturning the residual metal to the cathode 28. The method of makingalkali-metal cyanogen compounds consisting in electrolyzing a moltencompound of the alkalimetal, alloying the separated alkali-metal with acathode metal, removing the alloyed cathode metal and the alkali-metal,separating the alkali-metal as a metal per se from the alloy, convertingthe soeseparated alkalimetal to an alkali-metal cyanogen compound bytreatment with nitrogenous and carbonaceous matter and returning theresidual metal to the cathode.

29. The method of making cyanogen compounds-consisting in electrolyzinga molten compound of a metal capable of forming nitrogen compounds,alloying the separated metal with a cathode metal, removing the alloyedfirst mentioned metal and cathode metal, separating as a metal per-8ethe constituent metal of said alloy which is capable of forming nitrogencompounds, from said .alloy and converting said separated metal to acyanogen compound bytreatment with nitrogenous and carbonaceous matter.

30. The method of making alkali-metal cyanogen compounds consistinginforming a mass of molten matter, one constituent of which is thealkali-metal of an alkali-metal compound to --be formed, byelectrolyzing a molten salt-of said alkali-metal and depositing the saidalkali-metal electrolytically into a body of molten cathode material,treating the said massof molten matter to separate at least a part ofthe so-incorporated alkalimetal therefrom as a metal per se andconverting said separated part into a cyanogen compound by reacting thesame with nitrogenous and carbonaceous matter.

31. The method of making cyanogen compounds consisting in forming a massof molten matter, one constituent of which is a metal and anotherconstituent of which is I a cathode material by electrolyzing a moltensalt of the said metal and depositing. the

said metal electrolytically into a molten bodyof said cathode material,treating the said mass (qt molten material to separate at least a partof the so-incorpprated metal there from as a metal per ac and convertingsaid separated metal into a cyanogen compound by reacting upon saidmetal with nitrogenous and carbonaceous matter.

32. The method oi making cyanogen compounds consisting inelectrolytically liberating a metallic element capable of formingnitrogen compounds, in a chamber containing molten cathode metal to forman alloy,

' the cathode.

naraarro comprising said element and said cathode metal, conveying saidliberated element while alloyed with said cathode metal to a secondchamber, separating said element as a metal per $6 from said alloy andeffecting a reaction in which said separated metallic element, carbonand nitrogen participate.

33. The method of making cyanogen com pounds consisting inelectrolytically liberating a metallic element capable of formingnitrogen compounds, in a chamber containing molten cathode metal,conveying said liberated element while. alloyed with said cathode metalto a .second chamber, separating said element as a metal per 86' fromsaid alloy, effecting areaction in which thesaid separated element,carbon and nitrogen participate and returning the impoverished alby tosaid first mentioned chamber.

34. In a method of making nitrogen compounds continuously electrolyzinga molten compound of a metal capable of forming nitrogen compounds,alloying the separated compound of a metal capable of forming nitrogencompounds, alloying theseparated metal with a molten cathodemetal,-removin'gthe molten alloy, separating as a metal per se invaporous form the constituent metal of said alloy which is capable offorming nitrogen compounds, from said alloy and returning the residualmetal to the cathode.

36. In a method of making nitrogencompounds continuously electrolyzing amolten compound of a metal capable of forming nitrogen compounds,alloying the. separated metal with a molten cathode metal, removing andheating the molten alloy, separating as a metal per se in ,vaporous formthe const tuent metal of said alloy which is capable of forming nitrogencompounds, from said alloy and returning the residualv metal to the.cathode.

i 37. Tn a method of making nitrogen compounds continuouslyelectrolyzinga molten compound of aunetalcapable of forming nitrogen componds with amolten metal cathode, removing the molten cathode product,

separating as a metal per se in vaporous F .4. 1' rorm the constituentmetal of said cathode product which is capable of forming nitro- I 4 gencompounds, from said cathode product and returning the residual moltenmetal to 36 In a method of making nitrogen commiemo compound of a metalcapable of forming nitrogen compounds with a molten metal cathode,removing and heating the molten cathode product, separating as a metalper se in vaporous form the constituent part of said cathode productwhich is capable of forming nitrogen compounds, from said cathodeproduct and returning the residual molten metal to the cathode.

specification in the presence of two subscribmg Witnesses.

HANS EUEESTEELING. HERBERT PHELIPP.

Witnesses:

L. M. Eossr, E. Reps. I

